Apparatus for improving flavor constituents



Oct. 18, 1966 E. J. KELLY APPARATUS FOR IMPROVING FLAVOR CONSTITUENTS 2Sheets-Sheet l Original Filed Dec. 5, 1960 INVENTOR. [o6-,oe J KELLY .N.www

Ost. 18, 1966 E. J. KELLY 3,280,008

APPARATUS FOR IMPROVING FLAVORCONSTITUENTS Original Filed Deo. 5. 1960 2Sheets-Sheen?I 2 l s u b 2 E 3 i l INVENTOR. Evene el. KELLY u BY a,vw/f, /wufm l1 ,Urfa/eusse.

United States Patent O 3,280,008 APPARATUS FOR IMPROVING FLAVORCONSTITUENTS Edgar J. Kelly, Placentia, Calif., assignor to Libby, Mc-

Neill & Libby, Chicago, Ill., a corporation of Maine Originalapplication Dec. 5, 1960, Ser. No. 73,742, now

Patent No. 3,223,533, dated Dec. 14, 1965. Divided and this applicationSept. 3, 1965, Ser. No. 496,216

3 Claims. (Cl. 202-160) This application is a division of application73,742 filed December 5, 1960, now Patent 3,223,533. The presentinvention is directed to a system or apparatus for separating thecharacteristic odor and flavor constituents from aqueous sourcematerials generally derived from fruit, berries, beverage materials,such as tea and coffee, etc. The invention is also directed to specificconditions and arrangements of elements for the production of a newconcentrate or distillate containing the flavor and aroma constituentsin very large proportion or high concentration. The present invention isalso directed to apparatus for removing traces of `oily constituentswhich contaminate the flavor and aroma constituents.

For many years it has been recognized that fresh fruit and vegetablejuice contained avoring and aromatic constituents which are extremelycharacteristic of the particular fruit, plant extract or the like. Ithas also been recognized that the natural, fresh flavor and aroma offruit, berries, tea, coffee and other foods are deleteriously affectedby the normal concentrating, heating and sterilizing steps, with cookedand off flavors and with a loss of the aroma and avor whichcharacterizes fresh, mature fruit. Some attempts have been made in thepast to recover the relatively volatile avors and components found inplant products for the purpose of reintroducing them into the finalconcentrate or canned, cooked or sterilized fruit in order to impartthereto the flavor and aroma of the fresh, natural fruit.

Prior attempts to obtain a fraction in which it was hoped that theilavoring and aromatic constituents would be present in concentratedquantity were not successful and were fallacious in their method ofoperation. Prior workers in this art appeared to be confused and lookedfor an oily material as a source of the flavor. The present inventionobtains the flavoring and aromatic constituents in a non-oily,water-soluble and miscible form which is virtually colorless,transparent, mobile, burns with a clear blue flame and has a remarkablylow freezing point, well below 100 C. and as low as 180 C.

In addition directly contrary to the teaching of the prior art, it hasbeen found that oily contaminants are present with the flavor andaromatic constituents in certain citrus products, which even inextremely small proportions impart unpleasant taste and odorcharacteristics. Also it has been found that the avor concentrate itselfis a solvent for such oily contaminates so that if the oilyPcontaminants are not removed prior to concentration of the llavor andodor constituents lthen separation becomes extremely diilicult if notimpossible.

One of the reasons for the failures of the prior art was the fact thatthe prior workers did not realize the importance of maintainingconditions of temperature and pressure below 65 C. and 190 mm. of Hgwhen dealing with fruit juices, citrus juices and other sourcematerials. It has been found that the conditions of operation should besuch as to prevent or minimize hydrolysis of the esters and ethers ofacetic acid into acids, alcohols and secondary reaction products. It hasalso been discovered that the esters and ethers of acetic acidconstitute important components which impart the characteristic fresh,natural flavor and aroma elements to the concentrate and to the3,280,008 Patented Oct. 18, 1966 ICC products in which it issubsequently used; colorimetric determination of the ethyl ester ofacetic acid (ethyl acetate) content of a concentrate provides a readymode of evaluation.

Although some prior patentees have referred to what they termed a 100fold essence which they allegedly obtained, such term had no truemeaning other than the volume of the condensate taken out of the systemwas 1/100 of the juice fed into the system. For example, Patent No.2,457,315 speaks of pumping g.p.h. of apple juice into a single stageevaporator, evaporating 10% of such juice, passing the vapors into afractionating column and condensing the vapors from such column, all atatmospheric pressure. Uncondensed gases were vented from the condenserand the condensate was drawn off at 1/100 of the rate at which freshjuice was fed into the evaporator, this condensate being termed a 100fold essence. It is evident that in such process the condenser would befed with vapors composed essentially of water and therefore thecondensate would also consist essentially of water since the water willbe condensed first. The mole fraction or concentration of the flavorconstituents in vapors sent to such prior condenser is far below 0.5%and the vapors would exhibit all ofthe properties of water vapor. Thepartial pressure of the volatile constituents at no time approachsaturation pressures. At no time would the prior patentees eliminate thewater and then condense the more volatile constituents under conditionswhich effectively utilized partial pressure phenomena and Daltons law.Dew point conditions (with respect to the flavoring and aromaticconstituents) were never reached; the mixtures of air, gases and vaporssent to the con-denser contained excessive amounts of water vapor. As aresult, the so-called 100 fold essence was simply a mathematical andvolumetric determination and did not actually contain any appreciablyincreased quantity 0f flavoring components.

The fallacy of the prior method of identifying the essence becomesapparent when one considers that orange juice appears to contain onlyabout 30 p.p.m. of true essence, so that only about 1.5 to 1.6 lbs ofwaterfree essence can be obtained from 52,000 lbs. of citrus juice. Theproducts made by the apparatus of this invention actually contain onethousand times as much avoring constituents as the original sourcematerial or juice, even in the unpuried, aqueous solution form in whichthey are normally obtained. Moreover, it is to be remembered that ethylacetate has a vapor pressure of 760 mm. absolute at about 77 C., whereaswater at the same temperature has a vapor pressure of 7 lbs. gauge.

Contrary to prior suggestions that the concentrated or flavor-strippedjuice be used as an absorbent or scrubber for the non-condensed gases orvapors prior to venting such residual gases (in an attempt to recoversome of the ilavoring components from said gases), it has been foundthat such flavor-stripped juices are not good absorbents; instead, pureWater (or dilute, aqueous solutions of ethyl alcohols or sucrose) havebeen found much more effective. Also contrary to prior practice whichwas concerned solely with removing water in order to obtain a smallvolume of liquid to be fractionally distilled, the present inventionafter initially obtaining a small volume liquid actually adds water toseparate the oily contaminants prior to fractional distillation sincesimple condensation does not separate the oily contaminants from theflavor constituents.

` fruits, berries, aqueous extracts of tea leaves, roasted and groundcoffee, etc.) by conducting all of the operations under temperature andpressure conditions which will not cause hydrolysis of esters of aceticacid, the temperatures not exceeding 65 C. and preferably being below 43C. and absolute pressures not over 190 mm. of Hg and preferably as lowas 30 mm. Hg. Any such source material in the form of water vapor andnon-condensable gases containing minute quantities of volatile odor andflavor constituents is subjected to -a temperature below `about 43 C.and an absolute pressure of not over 115 mm. Hg in a condensation zoneto condense not less than 70%, and preferably 80% by weight of water-contained in said source material. After the water has been separa-tedfrom the residual vapors and gases, such vapors and gases are subjectedto dew point conditions for flavor and odor constituents and are readily-condensed in accordance with Daltons law. These flavor and odorconstituents are obtained in the form of aqueous solutions having thecharacteristics described hereinbefore containing in excess of 40 gramsper liter of such constituents. Ordinarily, the final product contains30,000 to 60,000 ppm. of the volatile `flavor-and aroma-impartingconstituents, this being a readily handled and utilized product which isnot as unstable as the pure essence; more concentrated forms have to behandled at very low ltemperatures because of their volatile character.

When the source material in the form of a gaseous mixture of water vaporand odor and flavor constituents contains traces of oily contaminants,it is rst scrubbed with chilled water. Then it is cooled and scrubbedagain with chilled water. The oily contaminants are then removed fromthe scrub water. The water yand scrubbed gaseous mixture are thenfractionally distilled to produce the gaseous mixture from which theflavor and odor constituents may be fractionally condensed.

It is an object of the present invention, therefore, to disclose andprovide means whereby concentrated distillates or produ-cts containingilavorand aroma-imparting constituents may be derived from variousaqueous media.

A further object of the present invention is to provide means wherebyoil-free avor and odor constituents may be separated from a gaseousmixture contamina-ted with oily constituents.

Those skilled in the art will readily appreciate various other objectsand advantages from the description of an exemplary arrangement ofapparatus in which the process may be carried out in the treatment ofcitrus juices. The appended diagrammatic representation of anarrangement of equipment, FIGS. Il and 2, is directed to the recovery ofan essence composed largely of odor and flavor constituents of the-character described hereinbefore. FIG. 3 is a diagrammatic`representation of an arrangement of equipment for the recovery offlavor and odor constituents contaminated by traces of oilyconstituents. l In the exemplary form of apparatus shown in the appendeddiagram FIG. 1, fresh citrus juice may be introduced into the lirst of apair of multiple effect evaporators 1 and 1 and a concentrated juice(from which 15% to about 20% of original water has been removed) isdischarged from the second evaporator. Water vapors from the secondevaporator may be sent by line 2 to condenser 2 and its condensate isnormally sent t-o waste. Non-condensable gases from 1 are sent to 1';non-condensable gases from 1 and condenser 2 are sent by lines 3 and 3to a fractionating column 6. Since the condensa-te from 1l contains some-avor and aroma constituent (this may also be true to a lesser degree ast-o condensate from 2), the condensate is pumped as by pump 5 and fed byline 4 to column 6. Those skilled in the art will understand thatsuitable supply of heat, valves, temperature and pressure indicatingdevices etc. are used and need not be shown in the diagram.

It is highly desirable that the multiple effect evaporators be operatedat as low temperature as possible, preferably below 65 C., althoughsomewhat higher temperatures may be employed. It is to be understoodthat the arrangement of evaporators or other equipment from which thenon-condensable gases and extracts or solutions are obtained are not anessential part of this invention; these preliminary units and operationswill vary in accordance with the material being treated; if, forexample, a coffee essence is to be obtained, no evaporators would beused, but instead, leaching tanks would -be employed for the purpose ofobtaining an aqueous extract of coffee, such extract being made at a lowtemperature of below about 65 C. and preferably at a temperature ofbelow about 43 C.

The equipment illustrated in the diagram lFIG. 1 and adapted to carryout the process herein disclosed comprises, in addition to thefractionating column 6, a primary overhead type of condenser indicatedat 12, a series of saturation component condensers indicated at 18 and20, -a scrubber indicated at 26 and a constant pressure chamberindicated at 30. It is to be understood that additional saturationcomponent condensers may be employed, the diagram being limited to thetwo, 18 and 20, only for purposes of simplification. The entire systemfrom the fractionating column 6 to the constant pressure chamber 30 ismaintained under a substantially uniform vacuum. `Uniform and constantvacuum conditions below about mm. Hg are preferably maintainedthroughout the system; it has been found `desirable to maintainpressures as low as 30 mm. Hg in the saturation component condensers 18and 20 and the scrubber 26. The desired vacuum conditions are attainedby connecting the outlet line B1 extending from the constant pressurechamber 60 to a suitable source of vacuum, such as a barometriccondenser, Isuitable pumps, ejectors or the like.

The fractionating column 6 is maintained with a bottom temperature ofnot over about 55 C., although temperatures as high as 65 C. may be usedin some instances. Temperatures at the top of the fractionating columnshould not exceed 43 C. and are preferably maintained on the order ofabout .v3-2 C.-33 C. A part of the -bottoms discharged from the bottomof the fractionating column y6 as by line 7 and sent to the pump 8 maybe recirculated through a reboiler 9 and returned to the fractionatingcolumn, as indicated. These bottoms may be discharged by the pump 8 towaste or other disposal.

The vapors from the fractionating column 6 are discharged by line 10Et-o the condenser 12. The temperature and pressure conditions within thecondenser 12 are such as to condense not less than about 70% by weightof water contained in the vapors submitted to such c-ondenser throughthe line 10. As previously indicated, the virtually constantsubatmospheric pressure is maintained throughout the system and suchpressure should be below about mm. Hg. In actual practice, pressures ofapproximately 50 mm. Hg to as low as 30 mm. Hg are employed; under suchpressure conditions the temperature within the condenser 12 ismaintained at between about 30 C. and 43 C. in order to thoroughlystrips the gases of at least 70% of their moisture content.

The condensed water is discharged from the overhead condenser 12 as byline 13 and the uncondensable components, residual vapors and gases, aredischarged as by lines 14 and 14 into the first of a series ofsaturation component condensers such as the condenser 18. A valve 15 isindicated in the line 14 and although normally kept open, may be used toslightly throttle the gases and assure condensation of the requiredamount of water in the condenser 12.

The condenser 18 is operated at a temperature of, say around 16 C.-18C., and gases which have not been condensed in the condenser 18 aredischarged by line 19 into the condenser 20, which in the example beinggiven, would now operate at a still lower temperature, say, atemperature of approximately 10 C. The odor and flavor constituentswhich have been condensed in condensers i18 and 20 are dischargedtherefrom by lines 18 and 20', respectively, into a manifold line 21,permitting these odor and avor constituents to be combined. Theuncondensed vapors and gases from con-denser 20 are then shown beingsent by line 22 to the scrubber 26. This scrubber also operates at thevery low pressure of 30 mm. to 50 mm. Hg and spray of scrubbing liquidsupplied thereto by line 23 is preferably chilled as by a chiller 24before introduced into the scrubber. As previously indicated, it isdesirable to use clean, pure Water as a scrubbing liquid and such watermay be supplied to the chiller 24 by means of pump 25 and line 23. T-heliquid from the scrubber 26, containing its absorbed and adsorbed odorand ilavor constituents, is discharged into the line 21. The stilluncondensed and uncondensable vapors or gases from the scrubber are nowdischarged as by line 27 into the constant pressure chamber 30. FIG. 2represents an enlargement of constant pressure chamber 30 and shows moredetails of its construction. This device insures constancy of vacuumthroughout the system and contains a body of water in its lower portion,together with a temperature control device indicated at 32 whichactuates a valve (or switch) so as to admit either steam or electriccurrent into a heating coil located in such body of water in the eventthe temperature of the body of water drops below a predetermined point.A float control is also provided (indicated at 33) for the purpose ofmaintaining a constant level of water in the device. As previouslyindicated, the outlet pipe 311 leading from the constant pressurechamber is associated with a suitable source of vacuum.

The condensates discharged from condensers 1S and 20 and the scrubber 26will contain the greatest concentrations of the odor and flavorconstituents. For example, when the system is operated on orange juice,the concentrations obtained will range from between about 10,000 p.p.m.to 150,000 p.p.m. The condensate from the pri- Vmary condenser 12 willalso contain some odor and flavor constituents but at a lowconcentration, say, only 100 to 200 p.p.m. Although the condensates andconcentrates from the condensers 18 and '20 and scrubber 26 may becombined in a line 21 and separately withdrawn as indicated by line 28through a pump 29 and sent to essence tanks, bottling, or the like, ithas been found desirable to combine these concentrates with thecondensate from t-he primary condenser 12 because of the relativelylarge amount of the condensate obtained from condenser 12 in comparisonwith the relatively small quantities (having high concentration of odorand flavor components) obtained from the condensers 18, 20, etc. FIG. ltherefore shows line 2-1 in communication with outlet line 13, all ofthe concentrates being sent through a pump 16 and then by line 17 tostorage.

In the specific embodiment of apparatus shown in FIG. 3, the arrangementof evaporators is the same as that used in FIG. l. However, thenon-condensable gases from evaporator 1 and condenser 2 are sent bylines 3y and 3 to a scrubber 40 rather than directly to fractionatingcolumn 6. Likew-ise the condensate from evaporator 1 and condenser 2 ispumped by pump 5 and line 4 to a centrifuge 62 rather than directly tofractionating column 6. The gaseous mixture entering scrubber 40 usuallycontains about 0.01% oily contaminants and 60% -water vapor but maycontain over 0.1% oily contaminants. Since the operating pressure ofscrubber 40 is preferably maintained at about l mm. Hg, IDaltons lawindicates that the partial pressure of the `oily contaminants is usuallyabout 0.001 mm. Hg assuming a concentration of 0.01%. At such extremelylow partial pressures, it can be seen that extremely low temperatureswould have to be attained in order to simply condense the oilycontaminants. This point is emphasized by the fact that the oilycontaminants appear to be somewhat more volatile than water and thusmore diiicult to condense. Hence scrubber 40 while it does remove asmall part of the oily contaminants serves primarily to increase theirconcentration by removing other components of the gaseous mixture. Bycharging chilled water at about 35 F. at 41 and removing it at 40', alarge portion of the water vapor and other gaseous components areremoved so that the gaseous mixture leaving scrubber 40 through conduit42 usually contains about 1% oily contaminants and 10% Water vapor.

The gaseous mixture is pumped through scrubber 40 and conduit 42 bymeans of a steam jet pump 43 which is fed by steam line 44. The steamjet pump is used to avoid further contamination of the gas mixture withoil. Also by placing t-he steam jet pump after a scrubber 40, the amountof gas to be pumped is minimized and consequently the amount of Wateradded to the gas mixture in the form of steam is minimized. However, thegaseous mixture leaving the steam jet pump 43- through conduit 43' atabout 40 C. and 30 mm.50 mm. Hg has oily contaminants in substantiallyreduced concentration and greatly increased water vapor concentrationi.e. it usually has approximately 0.1% oily contaminants and watervapor. Therefore the gaseous mixture is sent through condenser 45 wherea large portion of the Water vapor is condensed and removed along withother condensable components of the gaseous mixture through conduit 45'.The gaseous mixture leaving condenser 45 through conduit 46 consequentlyusually contains about 5% oily contaminants and 15% water vapor.

The gaseous mixture is` then sent through a scrubbercondenser 47 whereis it cooled to -about 35 F. by a coolant such as ammonia and scrubbedwith water. Because of the relatively high concentration of oilycontaminants in the scrubber-condenser 47 e.g. usually about 5% and theabsorbing effect of the scrub water, the water leavingscrubber-condenser 47 through conduit '47' usually contains about 5%oily contaminants. Such result can be understood since the operatingpressure of the scrubber condenser is usually `about 30 to 50 mm. Hg sothe partial pressure of the oily contaminants is at least about 1.5 rnm.Hg and hence their dew poin-t can be attained. The gaseous mixture isthen sent by conduit 48 from scrubbercondenser 47 to scrubber 49 for anal scrub with chilled water Iat Iabout 35 F. entering at 50. The scrubwater leaves scrubber 49 through conduit 48 to be reused inscrubber-condenser 47. The gaseous mixture leaving scrubber 49 throughconduit 51 to feed fractionatitng column 6 contains no ascertainableoily contaminants but still contains Ithe major portion of the flavorand odor constituents since they are present :in such smallconcentrations throughout the steps for removing the oily contaminants.

The scrub water from scrubber-condenser 47 is combined with thecondensate fro-m condenser 45 and the scrub water from scrubber 40 inconduit 61 and sent through cooler 60 to reduce resulting combinedliquid temperature to about 35 F. The combined liquid stream leavingcooler 60 contains only about 0.5% oily contaminants so the lowertemperature is preferred to facilitate separation. The liquid leavingcooler 60 through conduit 60 is combined with condensate from evaporator1 `and condenser 2 and Isent to a centrifuge 62 where about 99.9% of theoily contaminants are removed through conduit 63. The substantiallyoil-free aqueous solution leaving centrifuge 62 through conduit 64 ispumped by pump 65 through conduit 66 to a filter 67 where the lasttraces `of oily contaminants are removed. Pump 65 must n-ot beoil-lubricated since this would add additional oily contaminants. Onetype of pump which maybe used is a centrifugal pump with a mechanicalseal. Filter 67 may be a conventional filter with a filter aid such yasdiatomaceous earth s-o long as the eiective filter openings aresufliciently smaller than the oil globules in the aqueous solution e.g.filter openings lof `approximately 1 micron compared to oil globules ofapproximately 10- 100 microns. The aqueous solution leaving filter 67 byconduit 68 is then heated by heater 69 and sent to fractionating column6 through conduit 70.

The following data may be `of i-nterest in indicating the resultso-btained on orange juice where the fractionating tower 6 was fed withvapors and concentrate containing approximately 30 p.p.m. of the odorand flavor constituents and the entire .system was maintained at asubatmospheric pressure of 45 mm. Hg. The concentrate from the condenser12 maintained at a temperature of 38 C. contained about 100 p.p.m. ofthe essence and amounted to two gallons per minute; the condensate fromcondenser 18 (maintained .at a temperature of 16 C.) contained 20,000

4p.p.m. of lthe essence but the discharge amounted to only 0.1 gpm.; thecondensate from condenser 20 (maintained at a temperature ofC.)`contained 100,000 p.p.m. of essence discharged at the rate of 0.1gpm.; the scrubber 26, maintained at a temperature of -only 2 C.,accounted for 0.5 g.p.m. containing about 10,000 p.p.m. of essence.

As previously indicated, the temperature andpressure conditions withinthe entire system are such as to prevent or minimize hydrolysis of theesters and ethers of acetic acid into acids, alcohols and secondaryreaction products. A determination of the ethyl acetate content of theconcentrate or condensate is the simplest and most effective method ofdetermining the actual presence of the odor and flavor constituents andin evaluating such concentrates and essence and the reagents and methoddescribed in Patent 2,992,978 may be used.

The essence obtained from the juice of citrus fruits, crushed berriesand grapes, purees of deciduous fruits (such as apricots, apples, pears,peaches, etc.) can be used to impart a natural, fresh and characteristicflavor 'and aroma to food products and confections, ice cream,

etc. or reincorporated into the concentrated source material. Orangeessence obtained by this process can be 'added to concentrated orangejuice and convert the usual flat, cooked taste of reconstitutedbeverages made from such concentrates into beverages which cannot bedistinguished from natural fresh juice. Citrus essences obtained arefree from the terpene-like odors and flavors which characterize citrusoils. One of the important characteristics of the essences recovered bythis invention is stability upon storage; this may be due, in part atleast, to the fact that hydrolysis and decomposition are minimized atthe low temperature and pressure conditions, and to the fact that all ofthe constituents (including naturally contained stabilizing agents) arepresent in their usual,

' natural proportions.

Emphasis is again placed upon the necessity of maintaining low, uniformsubatmospheric pressures throughout 'the system composed of thefractionating tower and condensers and the conjoint use of progressivelylower temperatures at such uniform su-batmospheric pressure in order toobtain Ian essence containing the exceptionally high content of odorandflavor-imparting constituents in a form unaltered from that assumed bythe constituents in the fresh, natural source material. For best resultsthe maximum temperature of vapors should be lbelow about 55 C. at apressure of not above 115 mm. Hg absolute.

Piping between condensers, scrubbers and fractionating tower should besufficiently large to avoid any material Vprevents the barometriccondenser, ejector, purge or vacuum pump from dropping the pressure in12, 18, and 26 below Ithe desired pressure of, say, 50 mm. Hg. It is tobe noted that l lb. of air can carry about 10 lbs. of

'water vapor at 38 C. and about 50 mm. Hg, but will carry about 24 lbs.of water vapor at the same temperature if the pressure drops to 48 mm.Hg; l lb. of air can carry about 4 lbs. of water vapor at 38 C. and 56mm. Hg. These figures show the necessity of maintaining a uniformpressure, condensing and removing the major proportion of water from thegases and then decreasing the temperature to obtain the benefit of thechange in partial pressures and reach the dew point of the flavor andodor constituents. Although 1 lb. of air will carry 10 lbs. of watervapor at 50 mm. Hg and a temperature of 38 C., only 0.2 lb. of watervapor can be carried by l lb. of air at 50 mm. Hg and a temperature of16 C.; at 10 C. and the same pressure, the water vapor capa-city of airis down to about 0.14 lb. Applicant therefore utilizes a mode ofoperation which distinguishes from all prior methods, and is able toobtain condensed essence containing in excess of 30,000 p.p.m. of thedesired constituents in commercial installations.

It must also be emphasized that when oily contaminants are present inthe gaseous mixture even in extremely low concentrations, they must beremoved. Prior practice failed to remove such oily contaminants not onlybecause the result they produced i.e. ofi-flavored concentrate was notrecognized but also their high volatility and low concentrationprevented their removal by simple condensation or scrubbing. The presentinvention by first increasing the concentration of the oily contaminantsin the gaseous mixture containing the odor and flavor constituents andthen scrubbing the gaseous mixture at a low temperature is able toremove the oily contaminants. The actual equipment necessary to obtainthis result can vary considerably from that schematically illustrated.For example, the steam jet pump with its associated condenser isunnecessary where a suicient vacuum can be maintained by the vacuum pumpconnected to the outlet line 31 such as when a barometric condenser isused with a relatively high operating temperature. Also the finalscrubber is unnecessary where the scrubbercondenser is sufiicientlylarge and the scrubber-condenser itself may be replaced by two pieces ofequipment i.e. a scrubber and a condenser. However the combination ismore economical and efficient. Of course, if the temperature of thegaseous mixture leaving the first scrubber is sufficiently loweg.approximately 35 F. because of entering at a low temperature and thegaseous mixture goes directly to a second scrubber then condenserbecomes unnecessary since its function has already been performed byusing the low entering temperature.

The essence of coffee, tea, cacao beans, and other condiments and foodproducts can be obtained by leaching the ground source materials withwater at a temperature below about 30 C.-35 C. and then supplying suchaqueous infusions to the fractionating tower and its associated systemof condensers under the conditions hereinbefore described. Even in thecase of coffee, the resulting essence is a colorless, clearwater-miscible, mobile and volatile liquid of extremely low freezingpoint; a room is filled with the aromatic and stimulating fragrance offreshly percolating coffee when the stopper is removed from a smallbottle of such essence. Alkaloids are absent and such coffee essence maybe used in making flavorful coffee by addition to any inocuous, suitablycolored aqueous solution.

The equipment employed in the performance of the methods hereindisclosed can vary greatly from that schematically illustrated.Attention is called to the fact that each of the condensers and chillersis provided with suitable heat exchange devices supplied withcold water,brine or refrigerant under automatic temperature-responsive controls.Those skilled in the art can readily construct the equipment in thelight of this invention for any given volume of vapors andnon-condensable gases per hour, and evaluate the resulting essenceconcentrates by the test method herein referred to.

I claim:

1. A system for separating the oil vapor contaminates from a gaseousmixture containing water vapor and flavor and odor constituents and lessthan 0.1% oily contaminates whereby the deleterious effect of said oilycontaminates on said flavor and odor constituents is avoided comprising:a scrubbing means for contacting said gaseous mixture with a body ofaqueous absorbent including means for supplying gaseous mixture thereto,means for withdrawing gaseous mixture therefrom, means for supplyingscrubbing water thereto and means for withdrawing scrubbing watertherefrom; a scrubber-condenser means operatively connected to the meansfor withdrawing gaseous mixture from said scrubbing means includingmeans for supplying cooling fluid thereto, means for withdrawing coolingfluid therefrom, means for supplying scrubbing water thereto and drawingsaid gaseous mixture therefrom, means for withdrawing scrubbing watertherefrom, means for supplying said gaseous mixture thereto and meansseparating said cooling fluid from said gaseous mixture and scrubbingwater; and an oil removing means operatively connected to the combinedliquid outlets of said scrubber and scrubber-condenser.

2. A system for pre-treating an aqueous feed material containingvolatile flavor and odor constituents and also less than 1% unstableyoily contaminates which tend to impair the quality of the iiavor andodor constituents to remove substantially all of such unstable oilycontaminates without damage to the avor and odor constituentscomprising: means for vaporizing said aqueous mixture at a temperaturenot in excess of about 65 C. to form a gaseous mixture containing watervapor, flavor and odor constituents and not more than about 0.1% of saidunstable oily contaminates; a first condensing means operativelyconnected to the vapor outlet of said vaporizing means for removing aportion of the water vapor from said gaseous mixture; a first scrubbingmeans operatively connected to the vapor outlet of said vaporizing meansand said condensing means including a vapor inlet for supplying saidgaseous mixture to the lower portion thereof, a vapor outlet from theupper portion thereof, a scrubbing water inlet in the upper portionthereof, and a scrubbing water outlet in the lower portion thereof; asteam jet pump operatively connected to the vapor outlet of said firstscrubbing means for moving said gaseous mixture through said firstscrubbing means; a second condensing means operatively connected to thevapor outlet of said steam jet pump for removing a portion of the watervapor from said gaseous mixture; a scrubber-condenser means operativelyconnected to the vapor outlet of said second condensing means includinga cooling fluid inlet in the upper portion thereof, a cooling tiuidoutlet in the lower portion thereof, means for supplying scrubbing waterto and withdrawing said gaseous mixture from the upper portion thereof,a vapor inlet for supplying said gaseous mixture to the lower portionthereof, a scrubbing water outlet in the lower portion thereof and meansseparating said cooling uid from said gaseous mixture and scrubbingwater; a second scrubbing means operatively connected to the means forsupplying scrubbing Water to and withdrawing gaseous mixture from saidscrubber-condenser including means for supplying said gaseous mixture toand withdrawing scrubbing water from the lower portion of said secondscrubbing means, a vapor outlet from the upper portion thereof and ascrubbing water outlet inlet in the upper portion thereof; and a singleoil-removing means operatively connected to the combined liquid outletsof said scrubber, condensers and scrubber-condenser. v

3. A system as stated in claim 2 wherein said oilremoving meanscomprises a cooler operatively connected to the combined liquid outletsof said scrubbers, condensers and scrubber-condenser, a centrifugeoperatively connected to the outlet of said cooler, a pump operativelyconnected to the aqueous outlet of said centrifuge, a lter operativelyconnected to the outlet of said pump and a heater operatively connectedto the outlet of said filter.

References Cited by the Examiner UNITED STATES PATENTS 2,406,375 8/1946Hoyte 202-161 2,625,505 l/l953 Cross 203--42 2,680,708 6/1954 Cook202-186A 2,890,961 6/1959 Davis 99--205 2,992,978 7/ 1961 Kelly 202--186NORMAN YUDKOFF, Primary Examiner.

F. E. DRUMMOND, Assistant Examiner.

1. A SYSTEM FOR SEPARATING THE OIL VAPOR CONTAMINATES FROM A GASEOUSMIXTURE CONTAINING WATER VAPOR AND FLAVOR AND ODOR CONSTITUENTS AND LESSTHAN 0.1% OILY CONTAMINATES WHEREBY THE DELETERIOUS EFFECT ON SAID OILYCONTAMINATES ON SAID FLAVOR AND OFOR CONSTITUENTS IS AVOIDED COMPRISING:A SCRUBBING MEANS FOR CONTACTING SAID GASEOUS MIXTURE WITH A BODY OFAQUEOUS ABSORBENT INCLUDING MEANS FOR SUPPLYING GASEOUS MIXTURETHEREFROM, MEANS FOR SUPWITHDRAWING GASEOUS MIXTURE THEREFROM, MEANS FORSUPPLYING SCRUBBING WATER THEREFROM; A SCRUBBER-CONDENSER MEANSSCRUBBING WATER THEREFROM; A SCRUBBER-CONDENSER MEANS OPERATIVELYCONNECTED TO THE MEANS FOR WITHDRAWING GASEOUS MIXTURE FROM SAIDSCRUBBING MEANS INCLUDING MEANS FOR SUPPLYING COOLING FLUID THERETO,MEANS FOR WITHDRAWING COOLING FLUID THEREFROM, MEANS FOR SUPPLYINGSCRUBBING WATER THERETO AND DRAWING SAID GASEOUS MIXTURE THEREFROM,MEANS FOR WITHDRAWING SCRUBBING WATER THEREFROM, MEANS FOR SUPPLYINGSAID GASEOUS MIXTURE THERETO AND MEANS SEPARATING SAID COOLING FLUIDFROM SAID GASEOUS MIXTURE AND SCRUBBING WATER; AND AN OIL REMOVING MEANSOPERATIVELY CONNECTED TO THE COMBINED LIQUID OUTLETS OF SAID SCRUBBERAND SCRUBBER-CONDENSER.